反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 0.90 g of 2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-6-benzyloxypyridine, 0.1 g of 10% palladium/carbon and 5 ml of ethyl acetate was stirred for 3 hours at room temperature under hydrogen atmosphere. The reaction system was purged with nitrogen, then, the reaction solution was filtrated through Celite, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography to obtain 0.60 g of 6-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-pyridone. 1H-NMR(CDCl3/250 MHz) δ(ppm): 3.54 (s, 3H), 6.11 (d, 1H, J=7.9 Hz), 6.33 (s, 1H), 6.44 (d, 1H, J=7.8 Hz), 7.09 (d, 1H, J=6.7 Hz), 7.37 (d, 1H, J=8.9 Hz), 7.55 (dd, 1H, J=7.9,7.8 Hz)
WORKUP
后处理
- customThe reaction system was purged with nitrogen
- filtrationthe reaction solution was filtrated through Celite
- concentrationthe filtrate was concentrated